JPS58219201A - Measuring method for polymerization ratio - Google Patents
Measuring method for polymerization ratioInfo
- Publication number
- JPS58219201A JPS58219201A JP57102053A JP10205382A JPS58219201A JP S58219201 A JPS58219201 A JP S58219201A JP 57102053 A JP57102053 A JP 57102053A JP 10205382 A JP10205382 A JP 10205382A JP S58219201 A JPS58219201 A JP S58219201A
- Authority
- JP
- Japan
- Prior art keywords
- amount
- polymerization
- polymeric composition
- polymer composition
- volatile
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims description 13
- 229920000642 polymer Polymers 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 238000003908 quality control method Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000012882 sequential analysis Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/44—Resins; Plastics; Rubber; Leather
- G01N33/442—Resins; Plastics
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Polymerisation Methods In General (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は、重合率検出方法に係り、特に、ポリマーと七
ツマ−とからなる重合体組成物の重合反応途中の重合率
を検出するのに好適な重合率検出方法に関するものであ
る。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for detecting a polymerization rate, and in particular, a method for detecting a polymerization rate suitable for detecting a polymerization rate during a polymerization reaction of a polymer composition consisting of a polymer and a hexamer. It is related to.
重合体組成物の重合反応プロセスにおいては、その品質
管理を適正に行うため、重合反応途中の重合体組成物の
重合率をオンライン・リアルタイムで、かつ、精度良く
検出することが重要である。In the polymerization reaction process of a polymer composition, in order to appropriately control the quality thereof, it is important to accurately detect the polymerization rate of the polymer composition during the polymerization reaction online and in real time.
従来、重合反応途中の重合体組成物の重合率は、重合体
組成物の重合率と重合体組成物の粘度との間に、一定条
件（測定温度２重合温度、粘度測定時のすり速度等）の
もとて相関関係があることを利用し、重合体組成物の粘
度を測定した後に、予め実験尋で得られた重合体組成物
の重合率と重合体組成物の粘度との関係線図から重合体
組成物の重合率を検出する方法が慣用されている。Conventionally, the polymerization rate of a polymer composition in the middle of a polymerization reaction has been determined based on certain conditions (measurement temperature 2 polymerization temperature, slip rate at the time of viscosity measurement, etc.) between the polymerization rate of the polymer composition and the viscosity of the polymer composition. ), and after measuring the viscosity of the polymer composition, the relationship line between the polymerization rate of the polymer composition and the viscosity of the polymer composition obtained in advance in an experiment is calculated. A method of detecting the polymerization rate of a polymer composition from the diagram is commonly used.
このような重合率検出方法では、重合反応途中の重合体
組成物の重合率をオンライン・リアルタイムで検出でき
るものの、次のような欠点があった。Although such a polymerization rate detection method can detect the polymerization rate of a polymer composition in the middle of a polymerization reaction online and in real time, it has the following drawbacks.
（１）重合体組成物の粘度測定において、測定温度。(1) Measurement temperature in measuring the viscosity of a polymer composition.
阻
粘度測定時のすり速度を一定にすることがＰＪＩ６であ
るため、重合体組成物の重合率と重合体組成物の粘度と
の関係線図から重合体組成物の重合率な求める際に誤差
が生じ易くなり、したがって、重合反応中の重合組成物
の重合率を精度良く検出することができず、重合体組成
物の品質管理を適正に行うことができない。Since PJI6 is to keep the sliding speed constant when measuring the blocking viscosity, there is no error when determining the polymerization rate of the polymer composition from the relationship diagram between the polymerization rate of the polymer composition and the viscosity of the polymer composition. Therefore, the polymerization rate of the polymer composition during the polymerization reaction cannot be accurately detected, and the quality of the polymer composition cannot be properly controlled.
（２）測定温度１重合温度、粘度測定時のすり速度等が
変化すれば、重合率と粘度との関係も変化するため、重
合率と粘度との関係線図を作成するには、上記条件の組
合せによる膨大な量の重合率と粘度との相関データの蓄
積が必要となり、多大な時間と費用を要する、
なお、精度良く重合体組成物の重合率を検出する方法に
は、いわゆるガスクロによる分析方法があるが、この方
法で１！、重合体組成物の試料を溶剤に溶解させて試料
液とする溶解工程と、試料液を少量精度良くプノプリノ
グして分析器に注入するサンプル液検量工程と、分析器
に注入されたサンプル液をガス化した後に充填剤が装填
されたカラムを通気させカラム出口での流量を測定し検
量線として出力する分析工程を順次経て重合率が検出さ
れるため、重合反応途中の重合体組成物の重合率をオン
ライン・リアル”″″〉□イムで検出することができず
、したがって、重合体組成物の品質管理を適正に行うこ
とができないといった欠点があった。(2) Measurement temperature 1 If the polymerization temperature, sliding speed during viscosity measurement, etc. change, the relationship between polymerization rate and viscosity will also change, so to create a relationship diagram between polymerization rate and viscosity, the above conditions must be met. It is necessary to accumulate a huge amount of correlation data between polymerization rate and viscosity based on the combination of There is an analysis method, but this method is 1! , a dissolution process in which a sample of the polymer composition is dissolved in a solvent to obtain a sample liquid, a sample liquid calibration process in which a small amount of the sample liquid is accurately punoprinogged and injected into the analyzer, and a sample liquid injected into the analyzer is After gasification, the polymerization rate is detected through a sequential analysis process in which a column loaded with a packing material is aerated, the flow rate at the column outlet is measured, and a calibration curve is output. There was a drawback that the rate could not be detected online and in real time, and therefore the quality of the polymer composition could not be properly controlled.
本発明の目的は、上記した従来技術の欠点を解消するこ
とで１重合体組成物の品質管理を適正に行うことができ
る重合率検出方法を提供することにある。An object of the present invention is to provide a method for detecting a polymerization rate that can appropriately control the quality of a single polymer composition by eliminating the drawbacks of the prior art described above.
本発明の特徴は、重合反応途中の重合体組成物を定量抜
出して検量すると共に、該抜出し量と同量の重合体組成
物を揮発成分と不揮発成分とに分離した後に、該揮発成
分若しくは不揮発成分を検量し、検量された重合体組成
物の量と検量された揮発成分若しくは不揮発成分の量と
の比より重合体組成物の重合率を検出することで、重合
反応中の重合体組成物の重合率をオンライン・リアルタ
イムで、かつ、精度良く検出するようにしたことにある
。A feature of the present invention is that a quantitative amount of the polymer composition in the middle of the polymerization reaction is extracted and calibrated, and after separating the same amount of the polymer composition as the amount of the extracted amount into volatile components and non-volatile components, the volatile components or non-volatile components are extracted. By weighing the components and detecting the polymerization rate of the polymer composition from the ratio of the weighed amount of the polymer composition to the weighed amount of the volatile component or non-volatile component, the polymer composition during the polymerization reaction can be measured. The purpose is to detect the polymerization rate online, in real time, and with high precision.
本発明の一実施例を図面により駁明する。An embodiment of the present invention will be explained with reference to the drawings.
図面は、本発明を実施した重合率検出装置の系、□・
七
読図で、揮発成分・不揮発成分分離装ｒｊｌ（以下、分
離装置と略）１０には、定量供給装置１１７と定量抜出
装置、例えば、回転数で流量が決まるギヤポンプ１１と
が設けられ重合反応プロセスの、例えば、重合反応槽（
図示省略）に連結された導管加が連結されている。分離
装置１０と、分離装置１１０での操作圧力を揮発成分の
蒸気圧以下とする真空ポンプさ
校とは、凝縮ａ１３が設けられた導管２１で連結されで
いる。ギヤポンプ１１にはＡ／Ｄ変換器１４ ａが接続
された検量値ｒｌ １５ ａが連結され、また、凝縮器
１３に連結された導管ｎには、Ａ／Ｄ変換器１４ ｂが
接続された検量値［１５ｂが設けられている。Ａ／Ｄ変
換器１４ａ、１４ｂは、重合率指示装Ｗ１（以下、指示
装置と略）１６にそれぞれ接続されている。なお、検量
装置ｊ１５ａ、１５ｂｌま、例えば、流量計により流量
を測定し検量する装置、あるいは、一旦、タンクに溜め
た稜ロードセル等を用いて液の重量変化を測定し検量す
る装置、あるいは、液面計を用いて液面変化を測定し検
量する装置等で良く、また、指示装置１１１６は、検量
値の記憶１重合率の演算および重合率の指示機能を有し
ている。更に、分離装置ｌｌＯは、表面更新が良く短時
間で数百ｐｐｍまで脱揮できる薄膜蒸発＊ｉｌＦで良い
。The drawing shows the system of the polymerization rate detection device implementing the present invention, □・
In the diagram, a volatile component/non-volatile component separator rjl (hereinafter referred to as a separator) 10 is provided with a quantitative supply device 117 and a quantitative extraction device, for example, a gear pump 11 whose flow rate is determined by the number of revolutions. In the process, for example, a polymerization reactor (
A conduit connection (not shown) is connected. The separation device 10 and a vacuum pump that makes the operating pressure in the separation device 110 lower than the vapor pressure of the volatile components are connected by a conduit 21 provided with a condensate a13. A calibration value rl 15a connected to an A/D converter 14a is connected to the gear pump 11, and a calibration value rl 15a connected to an A/D converter 14b is connected to a conduit n connected to the condenser 13. A value [15b is provided. The A/D converters 14a and 14b are each connected to a polymerization rate indicator W1 (hereinafter abbreviated as an indicator) 16. In addition, the calibration device j15a, 15bl is, for example, a device that measures and calibrates the flow rate with a flow meter, or a device that measures and calibrates the change in weight of the liquid using a ridge load cell that has been stored in a tank, or It may be a device that measures and calibrates changes in the liquid level using a surface meter, and the indicating device 1116 has functions of storing calibrated values, calculating the polymerization rate, and indicating the polymerization rate. Furthermore, the separation device IO may be a thin film evaporator *ILF that has good surface renewal and can devolatilize up to several hundred ppm in a short time.
重合反応槽から定量供給袋［１７を介し導管加を仔で分
離装［１０に送給される途中の重合体組成物をギヤポン
プ１１で定量抜出し検量装置１５ ａで検量する。この
検量値１．ｔＡ／Ｄ変換器１４ ａで変換された後に指
示装置１６に入力される。また、分離装置１０には、ギ
ヤポンプ１１で抜出された量と同量の重合体組成物が定
量供給装置１７により供給され、この重合体組成物（ま
、真空ポツプ１２により揮発成分の蒸気圧以下の圧力で
操作される分離装置１０で短時間の内に揮発成分と不揮
発成分に分離される。A fixed quantity of the polymer composition being fed from the polymerization reaction tank to a separation vessel [10 through a fixed quantity supply bag [17] is drawn out using a gear pump 11 and calibrated using a measuring device 15a. This calibration value 1. After being converted by the A/D converter 14a, it is input to the indicating device 16. Further, the same amount of the polymer composition as the amount extracted by the gear pump 11 is supplied to the separation device 10 by the quantitative supply device 17, and the vapor pressure of the volatile components is increased by the vacuum pop 12. The separator 10 operated at the following pressure separates volatile components and non-volatile components within a short time.
この場合、不揮発成分１ま分離装置１０から排出され、
一方、揮発成分は分離装置１０から導管２１を経て凝縮
器１３に供給され、ここで凝縮、液化される。液化され
た揮発成分は、その量を検量装置 １５ ｂで検量され
た後に導管ｎを経て排出される。検量装置１５ ｂでの
検量値はＡ／Ｄ変換器１４ ｂで変換された後に指示装
ｒｙ！１６に入力される。指示装置１６でＩ！Ａ／Ｄ変
換器１４ａ、１４ｂでそれぞれ変換され入力された検量
値の比が演算され、その結果、重合組成物の重合率が指
示される。In this case, only one non-volatile component is discharged from the separator 10,
On the other hand, the volatile components are supplied from the separator 10 through the conduit 21 to the condenser 13, where they are condensed and liquefied. The amount of the liquefied volatile components is calibrated by the calibrating device 15b and then discharged through the conduit n. The calibration value in the calibration device 15b is converted by the A/D converter 14b and then sent to the indicating device ry! 16. I! on the indicating device 16. The ratio of the input calibration values converted by the A/D converters 14a and 14b is calculated, and as a result, the polymerization rate of the polymerization composition is indicated.
本実施例のような重合率検出方法では、重合体組成物の
揮発成分と不揮発成分との分離に要する時間並びに重合
率指示に要する時間が短時間で済むため、重合率をオン
ライン・リアルタイムで検出でき、また、重合体組成物
の量と重合体組成物から分離された揮発成分の量との直
接比をとるため、重合率を精度良く検出することができ
ると共に、従来技術のように重合率と粘度との関係線図
の作成およびそれに要する重合率と粘度との相関データ
の蓄積の必要もない。The polymerization rate detection method as in this example requires only a short time to separate the volatile and non-volatile components of the polymer composition and to indicate the polymerization rate, making it possible to detect the polymerization rate online and in real time. In addition, since the amount of the polymer composition and the amount of volatile components separated from the polymer composition are taken directly, the polymerization rate can be detected with high accuracy, and unlike the conventional technology, the polymerization rate can be detected with high accuracy. There is no need to create a relationship diagram between polymerization rate and viscosity and to accumulate correlation data between polymerization rate and viscosity.
なお、本実施例では、重合体組成物から分離された揮発
成分を検量し重合率を検出しているが、その他に、重合
体組成物から分離された不揮発成分を検量し重合率を検
出しても良い。また、重合体組成物は、本実施例の他に
重合反応プロセスラインから抜出すようにしても良い。In this example, the volatile components separated from the polymer composition were calibrated to detect the polymerization rate, but in addition, the non-volatile components separated from the polymer composition were calibrated to detect the polymerization rate. It's okay. Further, the polymer composition may be extracted from a polymerization reaction process line in addition to the present embodiment.
本発明は、以上説明したように、重合反応途中の重合体
組成物を定量抜出して検量すると共に、該抜出し量と同
量の重合体組成物を揮発成分と不揮発成分とに分離した
後に、該揮発成分若しくは不揮発成分を検量し、検量さ
れた重合体組成物の量と検量された揮発成分若しくは不
揮発成分の量との比より重合率を検出することで、重合
率をオンライン・リアルタイムで、かつ、精度良く検出
できるので、重合体組成物の品質管理を適正に行える効
果がある。As explained above, in the present invention, a polymer composition in the middle of a polymerization reaction is quantitatively extracted and calibrated, and after separating the same amount of the polymer composition as the extracted amount into volatile components and non-volatile components, By calibrating volatile components or non-volatile components and detecting the polymerization rate from the ratio of the calibrated amount of the polymer composition to the calibrated amount of volatile components or non-volatile components, the polymerization rate can be measured online and in real time. Since it can be detected with high accuracy, it has the effect of appropriately controlling the quality of the polymer composition.
図面は、本発明を実施した重合率検出装置の系統図であ
る。The drawing is a system diagram of a polymerization rate detection device implementing the present invention.
Claims (1)
ると共に、該抜出し量と同量の前記重２．合体組成物を
揮発成分と不揮発成分とに分離した後に、該揮発成分若
しくは不揮発成分を検量し、さ 検量された重合体組成物の量と、検量Ｘれた揮発成分若
しくは不揮発成分の量との比より前記水 重合体総量物の重合率を検出することを特徴とする重合
率検出方法。[Scope of Claims] 1. A quantitative amount of the polymer composition in the middle of the polymerization reaction is withdrawn and weighed, and the same amount of the polymer composition as the withdrawn amount is 2. After separating the combined composition into a volatile component and a non-volatile component, the volatile component or non-volatile component is calibrated, and the amount of the calibrated polymer composition and the calibrated amount of the volatile component or non-volatile component are calculated. A method for detecting a polymerization rate, comprising detecting the polymerization rate of the total water polymer based on the ratio.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57102053A JPS58219201A (en) | 1982-06-16 | 1982-06-16 | Measuring method for polymerization ratio |
| US06/503,349 US4515008A (en) | 1982-06-16 | 1983-06-10 | Polymerization rate detection method |
| DE3321654A DE3321654A1 (en) | 1982-06-16 | 1983-06-15 | METHOD FOR DETERMINING THE POLYMERIZATION LEVEL OF A POLYMER JOINT |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57102053A JPS58219201A (en) | 1982-06-16 | 1982-06-16 | Measuring method for polymerization ratio |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58219201A true JPS58219201A (en) | 1983-12-20 |
| JPH0129202B2 JPH0129202B2 (en) | 1989-06-08 |
Family
ID=14317020
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57102053A Granted JPS58219201A (en) | 1982-06-16 | 1982-06-16 | Measuring method for polymerization ratio |
Country Status (3)
| Country | Link |
|---|---|
| US (1) | US4515008A (en) |
| JP (1) | JPS58219201A (en) |
| DE (1) | DE3321654A1 (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4792908A (en) * | 1986-03-25 | 1988-12-20 | The Firestone Tire & Rubber Company | Method for controlling the mooney viscosity of compounded rubber formulations |
| US5100624A (en) * | 1990-06-04 | 1992-03-31 | Fmc Corporation | Apparatus for determining the stability of a peroxygen |
| US5655379A (en) * | 1995-10-27 | 1997-08-12 | General Electric Company | Refrigerant level control in a refrigeration system |
| CN101324470B (en) * | 2001-12-26 | 2011-03-30 | 加拿大马特森技术有限公司 | Temperature measurement and heat-treating methods and systems |
| CA2456482A1 (en) * | 2004-02-03 | 2005-08-03 | Bayer Inc. | Method and apparatus for controlling a polymerization reaction |
| US20100105847A1 (en) | 2006-01-24 | 2010-04-29 | Intertape Polymer Corp. | Plug flow bulk polymerization of vinyl monomers |
| US7906598B2 (en) * | 2006-08-30 | 2011-03-15 | Intertape Polymer Corp. | Recirculation loop reactor bulk polymerization process |
| CA2661231C (en) * | 2006-08-30 | 2015-12-01 | Intertape Polymer Corp. | Recirculation loop reactor bulk polymerization process |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2590436A (en) * | 1948-06-21 | 1952-03-25 | Shell Dev | Method for controlling chemical reactions |
| FR1507153A (en) * | 1965-07-26 | 1967-12-29 | Houilleres Bassin Du Nord | Method and apparatus for measuring the rate of thermal depolymerization of polymers |
| US3477819A (en) * | 1966-11-09 | 1969-11-11 | Gulf Research Development Co | Method for measuring extent of conversion in a chemical process |
| US3578404A (en) * | 1967-12-04 | 1971-05-11 | Dow Chemical Co | Automatic reaction rate apparatus |
| US3746509A (en) * | 1971-09-20 | 1973-07-17 | Nalco Chemical Co | Gas chromatography analysis of polymer |
-
1982
- 1982-06-16 JP JP57102053A patent/JPS58219201A/en active Granted
-
1983
- 1983-06-10 US US06/503,349 patent/US4515008A/en not_active Expired - Fee Related
- 1983-06-15 DE DE3321654A patent/DE3321654A1/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| DE3321654A1 (en) | 1983-12-22 |
| DE3321654C2 (en) | 1988-01-14 |
| US4515008A (en) | 1985-05-07 |
| JPH0129202B2 (en) | 1989-06-08 |
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